CN101618568B - Preparation method of superfine ceramic powder injection molding mixture - Google Patents
Preparation method of superfine ceramic powder injection molding mixture Download PDFInfo
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- CN101618568B CN101618568B CN2009100785805A CN200910078580A CN101618568B CN 101618568 B CN101618568 B CN 101618568B CN 2009100785805 A CN2009100785805 A CN 2009100785805A CN 200910078580 A CN200910078580 A CN 200910078580A CN 101618568 B CN101618568 B CN 101618568B
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Abstract
The invention discloses a preparation method of a superfine ceramic powder injection molding mixture, which belongs to the technical field of ceramic injection molding. The preparation method of the superfine ceramic powder injection molding mixture comprises the steps: carrying out ultrasonic dispersion or high-speed ball grinding dispersion and surface modification of submicron or nanometer level ceramic powder in surface active agent solution; evenly mixing the surface modified powder with a non water-solubility organic binding agent, a water-solubility organic binding agent and other additives in a mixer according to a specific order; injecting and molding obtained injecting and mixing material on an injection molding machine to obtain a blank body; and quickly degreasing the blank body by water in water and ethanol mixing solution with a certain proportion under a certain degreasing temperature system. The obtained water-degreased injection material has even mixture, high strength of a green blank and good fluidity. The degreasing method has high degreasing speed and good blank shape maintaining performance and avoids the defects of cracking, bubbling, and the like.
Description
Technical field
The invention belongs to the ceramic injection forming technical field, disclose a kind of preparation method and degreasing method that is used for superfine ceramic powder injection molding mixture.
Background technology
Ceramic injection forming is a kind of near-net-shape technology, can be continuous, efficient, low-cost high the and complex-shaped ceramic component of preparation size precision, its product is widely used in fields such as the energy, environmental protection, automobile, Aero-Space, chemical industry, biologic medical.
The water degreasing is an a kind of new chemical degreasing method of introducing the high polymer binder system with thermoplasticity and water-soluble feature in ceramic injection forming, advantages such as moulding preparation with degreasing efficient height, the control easily of degreasing defective, energy-conserving and environment-protective, suitable complicated shape and large-size ceramic parts, thereby drawbacks such as the degreasing speed that overcomes present hot degreasing generation is low, time length.But in manufacturing high reliability, high performance structure ceramic, often adopt superfine ceramic powder, and superfine ceramic powder is difficult in water degreasing binder system disperseing, reunites easily, cause injecting the mobile property decline of compound, lack of homogeneity.Simultaneously, the degreasing of single employing aqueous solvent, degreasing speed is wayward, causes defectives such as cracking bubbling easily.
Summary of the invention
The present invention is intended to develop the method for the ultra-fine pottery powder of a kind of suitable preparation injection molding mixture, and controlled, the manageable degreasing process of defective of exploitation degreasing speed.
The suitable superfine ceramic powder injection molding mixture that the present invention proposes comprises superfine ceramic powder and organic binder bond two parts: the percentage composition of ceramic powder is at 82-90%, and the organic adhesive agent content is at 10-18%.Superfine ceramic powder meso-position radius d
50Less than 1 μ m, the ceramic powder kind comprises zirconia, aluminium oxide, carborundum or silicon nitride.
Organic binder bond comprises following a few part:
Water-insoluble binding agent: 15-30%
Water-soluble binder: 45-65%
Surfactant: 1-3%
OPE: 5-15%
Low melting point organic matter: 5-10%
Plasticizer: 1-5%
Described water-insoluble binding agent comprises: TPO high polymer, polystyrene, polybutylene terephthalate (PBT), ethylene vinyl acetate copolymer, polymethyl methacrylate etc.Described water-soluble polymer comprises: polyethylene glycol, polyvinyl alcohol and polyethylene glycol oxide etc.Said plasticizer is a dibutyl terephthalate, DOTP and terephthalic acid (TPA) diamyl ester etc.Described low melting point filler is microcrystalline wax, Brazil wax or beeswax.The described surfactant that is used for the ceramic powder surface modification is stearic acid or oleic acid.
The present invention proposes following preparation method: at first surfactant stearic acid or oleic acid are dissolved in organic solvent, as ethanol, add ultrafine ceramic powder then.Carry out ultrasonic dispersion 5 minutes then, then magnetic agitation 2 hours in the water-baths of constant temperature 40 degree.So just can evenly coat the layer of surface activating agent at ceramic grain surface.Ceramic powder after the modification carries out at first adding non-water-soluble organic binder bond when mixing on muller, again 175-185 ℃ mixing about 10 minutes down; Mixing and temperature are reduced to about 130-150 ℃ then, add OPE, soluble organic adhesive and filler, mixing 15 minutes.At last the mixing roll temperature is reduced to 120 ℃, add plasticizer, mixing 10-15 minute, take off the compound cooling.
Material forming ceramic base substrate on injection (mo(u)lding) machine is closed in the injection that utilizes method disclosed by the invention to obtain, then with in the mixed solution of base substrate as for the second alcohol and water.The adding of ethanol can improve the speed of water degreasing.Be used for the mixed solution of the second alcohol and water of solvent degreasing, the ratio of ethanol is at 20-50%.The stage skimming temp system that the present invention proposes is, remains on 30-40 ℃ in previous hour temperature of degreasing, is increased to 50-60 ℃ in 2-5 hour follow-up temperature.Because along with going deep into of degreasing, degreasing speed descends, and in order to keep high degreasing speed, must improve skimming temp, but when temperature surpassed 60 ℃, distortion appearred in base substrate softening aggravation easily.
Embodiment one
Ceramic powder and organic binder bond ratio (percetage by weight) as shown in the table:
| Zirconia ceramics powder | Polyvinyl butyral resin | Polyethylene glycol | OPE | Stearic acid | Microcrystalline wax | Dibutyl terephthalate |
| 87 | 1.5-2.0 | 6.5-8.5 | 0.6-1.7 | 0.65 | 0.65-0.80 | 0.5 |
With preparation 1kg injection compound is example.The 6.5g stearic acid fully is dissolved in an amount of ethanolic solution, and 40 ℃ of ethanol temperature add the 870g zirconia ceramics powder in the solution then.Ultrasonic then dispersion 30 minutes, ultrasonic power stirred 2 hours then; Perhaps ball milling is 12 hours, rotating speed r/min.Then slurry drying, remove the zirconia ceramics powder that obtains surface modification behind the ethanol.The zirconia ceramics powder and the polyvinyl butyral resin of modification were mixed 10 minutes 175 ℃ of melting temperatures on mill or twin-screw mixer machine.Then the mixing roll temperature is reduced to 150 ℃, add OPE, Tissuemat E and microcrystalline wax, mixing 15 minutes.Then the mixing roll temperature is reduced to 120 ℃, add dibutyl terephthalate, mixing 15 minutes, cool off fragmentation then and obtain injecting compound.
Moulding 4.5mm * 6.0mm on injection (mo(u)lding) machine * 42.0mm base substrate falls in the mixed solution of base substrate as for alcohol and water then, alcohol concentration 30%, and solution temperature was 40 ℃ in preceding two hours, and the 3rd to 7 hour, solution temperature rose to 50 degree.Can slough polyethylene glycol more than 90% through degreasing in 7 hours.Base substrate can be proceeded Rapid Thermal degreasing and sintering.
Embodiment two
Ceramic powder and organic binder bond ratio (percetage by weight) as shown in the table:
| The aluminium oxide ceramics powder | Polymethyl methacrylate | High density polyethylene (HDPE) | Polyethylene glycol oxide | OPE | Stearic acid | Microcrystalline wax | Dibutyl terephthalate |
| 89 | 0.9-1.2 | 0.9-1.2 | 5.0-7.0 | 0.55-1.65 | 0.75 | 0.65-0.8 | 0.45 |
Alumina powder jointed surface modifying method is identical with example one.Mixed 10 minutes 180 ℃ of melting temperatures on the powder of surface modification and polymethyl methacrylate, polymethyl methacrylate mill or the twin-screw mixer machine.Then the mixing roll temperature is reduced to 130 ℃, add OPE, Tissuemat E and microcrystalline wax, mixing 15 minutes.Then the mixing roll temperature is reduced to 120 ℃, add dibutyl terephthalate, mixing 15 minutes, cool off fragmentation then and obtain injecting compound.
Moulding 4.5mm * 6.0mm on injection (mo(u)lding) machine * 42.0mm base substrate falls in the mixed solution of base substrate as for alcohol and water then, alcohol concentration 10%, and solution temperature was 30 ℃ in preceding two hours, and the 3rd to 7 hour, solution temperature rose to 40 ℃.Can slough polyethylene glycol more than 90% through degreasing in 7 hours.Base substrate can be proceeded Rapid Thermal degreasing and sintering.
Embodiment three
Ceramic powder and organic binder bond ratio (percetage by weight) as shown in the table:
| Silicon nitride ceramic | Polyvinyl butyral resin | Ethylene vinyl acetate copolymer | Polyethylene glycol | OPE | Stearic acid | DOTP |
| 83 | 1.3-2.2 | 0.8-1.6 | 8.5-11.1 | 0.7-2.0 | 0.8 | 0.7 |
The surface modifying method of beta-silicon nitride powder is identical with example one.The powder of surface modification and polyvinyl butyral resin, ethylene vinyl acetate copolymer mixed 10 minutes on mill or twin-screw mixer machine, 170 ℃ of melting temperatures.Then the mixing roll temperature is reduced to 130 ℃, add OPE and polyethylene glycol, mixing 15 minutes.Then the mixing roll temperature is reduced to 120 ℃, add DOTP, mixing 15 minutes, cool off fragmentation then and obtain injecting compound.
Moulding 4.5mm * 6.0mm on injection (mo(u)lding) machine * 42.0mm base substrate falls in the mixed solution of base substrate as for alcohol and water then, alcohol concentration 30%, and solution temperature was 40 ℃ in preceding two hours, and the 3rd to 7 hour, solution temperature rose to 50 ℃.Can slough polyethylene glycol more than 90% through degreasing in 7 hours.Base substrate can be proceeded Rapid Thermal degreasing and sintering.
Embodiment four
Ceramic powder and organic binder bond ratio (percetage by weight) as shown in the table:
| The silicon carbide ceramics powder | Polymethyl methacrylate | Ethylene vinyl acetate copolymer | Polyethylene glycol | OPE | Oleic acid | DOTP |
| 72 | 2.2-3.6 | 2.2-3.6 | 12.5-18.2 | 1.4-4.2 | 1.5 | 1.2 |
The process of oleic acid surface modification carbonization silicon ceramic powder is identical with the process in the example one.On mill or twin-screw mixer machine, mixing 10 minutes of the powder of surface modification with poly-polymethyl methacrylate, ethylene vinyl acetate copolymer, melting temperature 180 degree.Then the mixing roll temperature is reduced to 130 degree, add OPE and polyethylene glycol, mixing 15 minutes.Then the mixing roll temperature is reduced to 120 degree, add DOTP, mixing 15 minutes, cool off fragmentation then and obtain injecting compound.
Moulding 4.5mm * 6.0mm on injection (mo(u)lding) machine * 42.0mm base substrate falls in the mixed solution of base substrate as for alcohol and water then, alcohol concentration 40%, and preceding two hours solution temperature 50 degree, the 3rd to 7 hour, solution temperature rose to 60 degree.Can slough polyethylene glycol more than 90 through degreasing in 7 hours.Base substrate can be proceeded Rapid Thermal degreasing and sintering.
Claims (2)
1. the preparation method of a superfine ceramic powder injection molding mixture, it is characterized in that: described method is that superfine ceramic powder is disperseed and surface modification by ultrasonic dispersion or high speed ball milling in surfactant solution, ceramic powder after the surface modification and organic binder bond, and other additive is mixing even on mixing roll; The injection compound injection moulding on injection (mo(u)lding) machine that obtains obtains base substrate; Carry out the water degreasing then in water and alcohol mixed solution and under the skimming temp system; The weight percentage of described ceramic powder is 82-90%, and described organic binder bond weight percentage is 10-18%; Described organic binder bond contains:
Water-insoluble binding agent: 15-30%;
Water-soluble binder: 45-65%;
Surfactant: 1-3%;
OPE: 5-15%;
Low melting point organic matter: 5-10%;
Plasticizer: 1-5%;
Wherein, described water-insoluble binding agent comprises: TPO high polymer, polystyrene, polybutylene terephthalate (PBT), ethylene vinyl acetate copolymer, polymethyl methacrylate, polyvinyl butyral resin;
Described water-soluble binder comprises: polyethylene glycol, polyvinyl alcohol and polyethylene glycol oxide;
Described plasticizer is a dibutyl terephthalate, DOTP and terephthalic acid (TPA) diamyl ester;
Low melting point organic matter in the described organic binder bond is microcrystalline wax, Brazil wax or beeswax;
Described surfactant is stearic acid or oleic acid.
2. method according to claim 1 is characterized in that: described method also contains,
(1) ceramic powder of surface modification and non-dissolubility binding agent are mixing down at 175-180 ℃;
(2) melting temperature is reduced to 130-150 ℃, adds OPE, water-soluble binder and low melting point organic matter, mixes;
(3) when melting temperature is reduced to 120 ℃, add plasticizer, mix;
(4) the cooling fragmentation obtains compound.
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